CN106984253A - A kind of solid phosgene synthesizer and method - Google Patents
A kind of solid phosgene synthesizer and method Download PDFInfo
- Publication number
- CN106984253A CN106984253A CN201710289417.8A CN201710289417A CN106984253A CN 106984253 A CN106984253 A CN 106984253A CN 201710289417 A CN201710289417 A CN 201710289417A CN 106984253 A CN106984253 A CN 106984253A
- Authority
- CN
- China
- Prior art keywords
- reactor
- liquid
- inner chamber
- solid phosgene
- wavelength
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000007787 solid Substances 0.000 title claims abstract description 56
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 77
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000012546 transfer Methods 0.000 claims abstract description 6
- 238000010189 synthetic method Methods 0.000 claims abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 33
- 239000000460 chlorine Substances 0.000 claims description 33
- 229910052801 chlorine Inorganic materials 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 230000015572 biosynthetic process Effects 0.000 claims description 14
- 238000003786 synthesis reaction Methods 0.000 claims description 14
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 6
- 239000003999 initiator Substances 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000010276 construction Methods 0.000 abstract description 2
- 238000013461 design Methods 0.000 abstract description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 description 6
- 238000005660 chlorination reaction Methods 0.000 description 6
- UCPYLLCMEDAXFR-UHFFFAOYSA-N triphosgene Chemical compound ClC(Cl)(Cl)OC(=O)OC(Cl)(Cl)Cl UCPYLLCMEDAXFR-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 206010054949 Metaplasia Diseases 0.000 description 4
- 230000015689 metaplastic ossification Effects 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- UCVQOIPQDBZRMG-UHFFFAOYSA-N [C].COC(C=1C(C(=O)OC)=CC=CC1)=O Chemical compound [C].COC(C=1C(C(=O)OC)=CC=CC1)=O UCVQOIPQDBZRMG-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- -1 peroxide Compound Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/123—Ultraviolet light
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/0004—Processes in series
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a kind of solid phosgene synthesizer, it includes three reactors being sequentially connected in series from left to right, the height of three reactors is reduced successively from left to right, the heat transfer system of temperature and the adjustable wavelength installed in the inner chamber of the reactor and the ultraviolet source of power of the inner chamber of each reactor respectively including reactor housing, the liquid inlet opening for being arranged at the reactor housing, gas feed mouthful, material outlet and tail gas outlet, for controlling the reactor, the wavelength of the ultraviolet source is 200~400 nm.The device has the advantages that reasonable in design, simple in construction, easy to use；Meanwhile, the present invention also provides a kind of solid phosgene synthetic method, and this method can realize that solid phosgene serialization is kept the safety in production, and without using initiator, have broad application prospects.
Description
Technical field
The present invention relates to the synthesis of solid phosgene, in particular it relates to a kind of solid phosgene synthesizer and method.
Background technology
Triphosgene is also known as solid phosgene, and chemical name is double（Trichloromethyl）Carbonic ester.Triphosgene is white crystal, there is class
Like the smell of phosgene, molecular weight 296.75,78~81 DEG C of fusing point, boiling point is 203-206 DEG C, and density of solid is 1.78g/cm3, melt
Melt the g/cm of density 1.6293, dissolve in the organic solvents such as ether, tetrahydrofuran, benzene, ethane, chloroform.French chemist
Counclert just has been reported that for 1887 in synthesis of solid phosgene in 1880, its physical property, but its crystal structure is until 1971
Year is just reported.The research of the industrialized production of solid phosgene and application are just progressively developed after last century the eighties
Come, domestic industrial production and largely use, only less than the history of 20 years.
Research shows to have triphosgene in the presence of chlorion very safe quantify can be decomposed into phosgene, thus solves
The problem of phosgene of having determined can not be measured accurately during the course of the reaction.Up to the present, dimethyl carbonate（DMC）/ chlorinated with chlorine method
It is the unique industrial method for preparing solid phosgene.By raw material of dimethyl carbonate and chlorine in, the initiation of light, heat or initiator
The synthesis of agent chlorination reaction, this chlorination reaction is a kind of free chain reaction, and nuclear magnetic resonance research shows that chlorination is substep
Carry out.
The synthesis technique of solid phosgene can be divided into solvent method and substance law.
Solvent method synthesis technique uses carbon tetrachloride as solvent, and its advantage is that reaction temperature is relatively low, and utilization of Heat of Reaction is molten
The volatilization of agent is removed, and is reacted more steady.Azodiisobutyronitrile is used in Romanian Patent RO88608（AIBN）It is used as initiation
Agent prepares triphosgene, chlorine is led under the conditions of ultraviolet lighting and 20-80 DEG C 16 hours, and product yield is 95%, but initiator amount
It is excessive, easily explode, and used in last handling process a certain amount of CCL4, reactor efficiency is relatively low；And should
Technique is because of its later-period purification, and desolventizing is complex, and nineteen ninety-five developed country starts strict implement《Montreal Protocol book》
Development country starts to perform for 2005, and carbon tetrachloride is strictly limited and used because there is larger destruction to atmospheric ozone layer,
The technique can not be promoted.
Substance law realizes the complete chlorination of dimethyl carbonate under initiator effect, mainly there is two major classes：（1）Use peroxide
Compound, azo-initiator or the two with the use of trigger substitution reaction；（2）Use ultraviolet light-initiated substitution reaction.
The former is because of the consumption of initiator, and adding speed, temperature control is harsher, and the segment of initiator can be in the product
Retain, the purity, performance to product can produce certain influence.Yao Sheng etc.（《Hunan chemical industry》, 1999,29 (5)：20）With
Benzoyl peroxide（BPO）And the study on the synthesis of the triphosgene of the substance law of BPO/ photoreactivation initiation, find with BPO consumptions
Increase and the increase of luminous power, chlorination reaction are significantly accelerated, but BPO consumptions no more than 4 g/mol DMC, because excessive
BPO can promote triphosgene to decompose in the reaction.Taken in Chinese patent CN347870 fluorescence and ultraviolet light and in, low temperature mix
Chlorination reaction is completed under conditions of conjunction initiator, the whole process of reaction is divided into basic, normal, high temperature three phases by they, is obtained
Product close to sterling, 80-83 DEG C of fusing point, yield more than 90%, but method is excessively complicated, is not easy to industrial applications.
The latter using it is ultraviolet it is light-initiated there is larger industrial production advantage, but with ultraviolet light-initiated, light source is wanted
Ask strict.Existing process production capacity is smaller, and typically at 3000~5000 tons, unstable product quality is easily sent out in use
Raw blast.Therefore, how to realize solid phosgene safe and continuous metaplasia production and be urgently to be resolved hurrily ask without using organic initiators etc.
Topic.
The content of the invention
In view of this, present invention offer one kind is reasonable in design, simple in construction, can realize solid phosgene safe and continuous metaplasia
Production and the solid phosgene synthesizer and method for being without the use of organic initiators, to solve the above problems.
Specifically, the present invention is adopted the following technical scheme that：
A kind of solid phosgene synthesizer, it includes three reactors being sequentially connected in series from left to right, three reactors
Height is reduced successively from left to right, and each reactor includes reactor housing, is arranged at the liquid of the reactor housing respectively
The heat transfer of charging aperture, gas feed mouthful, material outlet and tail gas outlet, the temperature of inner chamber for controlling the reactor
System and adjustable wavelength and the ultraviolet source of power installed in the inner chamber of the reactor, the wavelength of the ultraviolet source is
200~400 nm；The material discharge of liquid inlet opening positioned at the middle reactor and the reactor positioned at left side
Mouth is connected；The liquid inlet opening phase of the reactor positioned at the material outlet of the middle reactor and positioned at right side
Connection.
It is 330~400 nm positioned at the wavelength of the ultraviolet source of the reactor in left side based on above-mentioned；Positioned at centre
The wavelength of the ultraviolet source of the reactor is 300~330 nm；Positioned at the wavelength of the ultraviolet source of the reactor on right side
For 280~300 nm.
Based on above-mentioned, the temperature positioned at the inner chamber of the reactor in left side is 35~50 DEG C；Positioned at the described anti-of centre
The temperature for answering the inner chamber of kettle is 50~65 DEG C；Temperature positioned at the inner chamber of the reactor on right side is 65~90 DEG C.
Based on above-mentioned, the reactor further comprises the liquid distribution trough installed in the reactor inner chamber, the liquid
Body distributor is connected with the liquid inlet opening；Wherein, the liquid distribution trough includes ring-shaped liquid distributor cavity, the ring
It is evenly distributed with shape liquid distribution trough cavity in the multiple fluid apertures communicated therewith, the fluid apertures and liquid guide flow pipe is installed.
Based on above-mentioned, the reactor further comprises the gas distributor installed in the reactor inner chamber, the gas
Body distributor is connected with the gas feed mouthful；Wherein, the gas distributor includes annular gas distributor cavity and uniform
The Unidirectional air outlet pipe on the annular gas distributor cavity is distributed in, the Unidirectional air outlet pipe includes and the gas distributor
The escape pipe body that is connected of toroidal cavity and be arranged at the escape pipe body the port of export sideboard, the activity
Baffle plate is hinged with the escape pipe body.
Based on above-mentioned, the reactor also include being installed on the agitator of the reactor housing tip, with the stirring
Device is connected and the agitating shaft positioned at the inner chamber of the reactor, the stirring vane that is installed on the agitating shaft.
Based on above-mentioned, the agitating shaft respectively with the straight line extended line of the liquid guide flow pipe and the Unidirectional air outlet pipe
Angle is 45o。
Based on above-mentioned, the liquid inlet opening and the tail gas outlet are respectively arranged at the upper of the reactor housing
Portion, the gas feed mouthful and the material outlet are respectively arranged at the bottom of the reactor housing, and in the reaction
With the liquid inlet opening, the tail gas outlet, the gas feed mouthful and the material outlet on the outside of still shell body
Control valve is separately installed with corresponding position.
Based on above-mentioned, the heat transfer system includes enclosing the heat-conducting layer located at the outer surface of the reactor housing, each described
Heat-conducting layer is respectively arranged with heat-conducting medium entrance and heat-conducting medium outlet.
A kind of solid phosgene synthetic method, carries out solid phosgene synthesis, it includes using above-mentioned solid phosgene synthesizer
Following steps：
First by positioned at the wavelength regulation of the ultraviolet source of the reactor in left side to 330~400 nm, then by dimethyl carbonate
It is passed through in the reactor in left side and uniformly mixes with chlorine, and temperature of the regulation in the reactor in left side
Degree, makes dimethyl carbonate and chlorine in 0.1~0.2 Mpa, 35~50 DEG C of 3~4 h of reaction, obtains mixed once liquid；
First will once it be mixed to 300~330 nm, then by described positioned at the wavelength regulation of the ultraviolet source of the middle reactor
Close liquid and chlorine is passed through positioned at the middle reactor and uniformly mixed, and temperature of the regulation in the middle reactor
Degree, makes the mixed once liquid and chlorine in 0.1~0.2 Mpa, 50~65 DEG C of 2~3 h of reaction, obtains secondary mixed liquor；
First by positioned at the wavelength regulation of the ultraviolet source of the reactor on right side to 280~300 nm, then will be described secondary mixed
Close liquid and chlorine is passed through the reactor positioned at right side and uniformly mixed, and temperature of the regulation in the middle reactor
Degree, makes the mixed once liquid and chlorine in 0.1~0.2 Mpa, 65~90 DEG C of 2~3 h of reaction, obtains liquid solid phosgene.
Compared with prior art, the present invention is with prominent substantive distinguishing features and significantly progressive, specifically, of the invention
The solid phosgene synthesizer of offer includes three reactors being sequentially connected in series, and the inner chamber of three reactors can be corresponded to admittedly
Each step of body optical self-encoding sets different reaction conditions, is easy to control the process of solid phosgene synthesis to carry out safe and continuous
Metaplasia is produced；One upper lateral part of each reactor is provided with liquid inlet opening, and a side lower part of the reactor is provided with gas
Charging aperture, the gas material and liquid material for facilitating access for the reactor is sufficiently mixed in the presence of agitating device, is promoted
The progress of reaction, improves reaction efficiency；It is additionally provided with tail gas outlet, the tail gas outlet and sets on each reactor
There is dump valve, the pressure of the inner chamber of the reactor can be adjusted by the dump valve；The inner chamber of each reactor
The ultraviolet source of different wave length is respectively arranged with, the wavelength and power of each ultraviolet source can be adjusted, easy solid light
The light source of different wave length is selected in gas building-up process in different steps；It is described anti-that each reactor is respectively arranged with control
The heat-insulation system of the inner chamber temperature of kettle is answered, the temperature to each reactor is controlled respectively, the different step of correspondence reaction.
The present invention also provides a kind of solid phosgene synthetic method simultaneously, and this method ultraviolet light-initiated is consolidated by simple
Body optical self-encoding, without using organic initiators, it is to avoid organic initiators residual in the product, improves the quality of product,
Energy resource consumption is reduced, generation production is reduced originally, realizes and realizes that solid phosgene safe and continuous metaplasia is produced；It is solid by strictly controlling
The reaction condition of each step of body optical self-encoding, greatly avoids the decomposition of reaction heat accumulation releaser material, improves production
Efficiency.Compared with existing solid phosgene synthesis technique, the present invention 1 ton of solid phosgene of synthesis, energy consumption reduction by 70%, product quality
There is lifting by a relatively large margin, have broad application prospects.
Brief description of the drawings
Fig. 1 is the structural representation of solid phosgene synthesizer described in the embodiment of the present invention 1.
Fig. 2 is the structural representation of reactor described in solid phosgene synthesizer described in embodiment 1.
In figure, 1. reactor housings；2. agitator；3. pressure gage；4. tail gas outlet；5. thermometer；6. liquid level gauge；7.
Liquid inlet opening；8. liquid distribution trough；9. ultraviolet source；10. heat-conducting layer；11. fix bar；12. agitating shaft；13. stirring vane；
14. gas feed mouthful；15. gas distributor；16. material outlet；17. heat-conducting medium entrance；18. heat-conducting medium is exported；21.
Positioned at the middle reactor；31. the reactor positioned at left side；41. the reactor positioned at right side.
Embodiment
Below by embodiment, technical scheme is described in further detail.
Embodiment 1
The present embodiment provides a kind of solid phosgene synthesizer, as shown in Figure 1 and Figure 2, a kind of solid phosgene synthesizer, and it is wrapped
Three reactors being from left to right sequentially connected in series are included, the height of three reactors is reduced successively from left to right, each reaction
Kettle includes reactor housing 1, the liquid inlet opening 7 for being arranged at the reactor housing 1, gas feed mouth 14, material row respectively
Outlet 16 and tail gas outlet 4, the heat transfer system of the temperature of inner chamber for controlling the reactor and installed in the reaction
The adjustable wavelength of the inner chamber of kettle and the ultraviolet source 9 of power；Liquid inlet opening 7 and position positioned at the middle reactor 21
It is connected in the material outlet 16 of the reactor 31 in left side；Positioned at the material outlet 16 of the middle reactor 21
It is connected with the liquid inlet opening 7 of the reactor 41 positioned at right side, so that three reactors are connected, carries out material
Conveying.
Specifically, the wavelength positioned at the ultraviolet source 9 of the inner chamber of the middle reactor 21 is 300~330 nm；Position
In the inner chamber of the reactor 31 in left side ultraviolet source 9 wavelength be 330~400 nm；The reactor positioned at right side
The wavelength of the ultraviolet source 9 of 41 inner chamber is 280~300 nm；Temperature positioned at the inner chamber of the reactor 31 in left side is 35
~50 DEG C；Temperature positioned at the inner chamber of the middle reactor 21 is 50~65 DEG C；The reactor 41 positioned at right side
The temperature of inner chamber is 65~90 DEG C；So that three reactors can be carried out under different wave length irradiation and condition of different temperatures
Chemical reaction, in favor of the control of reaction condition.
Specifically, the liquid inlet opening 7 is located at a upper lateral part of the reactor housing 1, the gas feed mouthful position
14 are provided with liquid distribution trough 8, institute at the top of a side lower part of the reactor housing 1, the inner chamber of the reactor housing 1
The bottom for stating the inner chamber of reactor housing 1 is provided with gas distributor 15；The liquid inlet opening 7 and the liquid distribution trough 8
It is connected, the gas feed mouthful 14 is connected with the gas distributor 15, so that liquid material passes through the liquid feedstock
After mouth 7, the inner chamber that the liquid distribution trough 8 is uniformly distributed in the reactor is flowed through, gas material passes through the gas feed
After mouth 14, the inner chamber that the gas distributor 15 is uniformly distributed in the reactor is flowed through.
Specifically, the liquid distribution trough 8 and the gas distributor 15 can be individually fixed in described by fix bar 11
The inner chamber of reactor.
Specifically, the liquid distribution trough 8 and the gas distributor 15 include an annular housing, the liquid point
On the annular housing of cloth device 8 liquid guide flow pipe is separately installed with uniform some fluid apertures, each fluid apertures；The gas distributor
Some Unidirectional air outlet pipes are evenly equipped with 15 annular housing, the Unidirectional air outlet pipe includes the annular with the gas distributor 15
Escape pipe body that cavity is connected and be arranged at the escape pipe body the port of export sideboard, the sideboard with
The escape pipe body is hinged, to avoid the Unidirectional air outlet pipe from being blocked.
Specifically, the tail gas outlet 4 is located on the top of the reactor housing 1, the tail gas outlet 4 and set
There is dump valve, so as to the air pressure of the inner chamber that adjusts the reactor；The liquid inlet opening 7, gas feed mouth 14 and institute
State material outlet 14 and be respectively arranged with control valve.
Specifically, the reactor also includes being installed on the agitator 2 on the top of reactor housing 1, the stirring dress
Put including be arranged at each inner chamber for being connected with the agitator 2 and being located at the reactor 1 agitating shaft 12, be installed on
Some stirring vanes 13 on the agitating shaft, the stirring vane 13 can be arranged at the middle part of the agitating shaft 12 according to demand
And bottom, so that the material to each height is stirred.
Specifically, the agitating shaft 12 respectively with the straight line extended line of the liquid guide flow pipe and the Unidirectional air outlet pipe
Angle is 45o。
Specifically, the heat transfer system includes enclosing the heat-conducting layer 10 located at the outer surface of each reactor housing 1, described
Heat-conducting layer 10 is respectively arranged with heat-conducting medium entrance 17 and heat-conducting medium outlet 18, so that heat-conducting medium is in the heat-conducting layer 10
Inner chamber is circulated, to control the inner chamber temperature of the reactor 1.
Specifically, thermometer 5, pressure gage 3 and liquid level gauge 6, the thermometer 5 are also respectively provided with each reactor
It is located at the top of the reactor 1 with the pressure gage 3, the liquid level gauge 6 is located at the side of the reactor；The thermometer
5th, the pressure gage 3 stretches into the inner chamber of the reactor, and the liquid level gauge 6 is connected with the bottom of the reactor, so as to
Measure temperature, pressure and the liquid level of the inner chamber of the reactor.
Embodiment 2
The present embodiment provides a kind of method for applying above-mentioned solid phosgene synthesizer to carry out solid phosgene synthesis, and it includes following
Step：
First by positioned at the wavelength regulation of the ultraviolet source of the reactor in left side to 345 nm, then by dimethyl carbonate and chlorine
It is passed through in the reactor in left side and uniformly mixes, and temperature of the regulation in the reactor in left side, make carbon
Dimethyl phthalate and chlorine react 3~4 h under the conditions of 0.1~0.2 Mpa, 37 DEG C, obtain mixed once liquid；
First by positioned at the wavelength regulation of the ultraviolet source of the middle reactor to 327 nm, then by the mixed once liquid and
Chlorine is passed through positioned at the middle reactor and uniformly mixed, and temperature of the regulation in the middle reactor, makes
The mixed once liquid and chlorine react 2~3 h under the conditions of 0.1~0.2 Mpa, 59 DEG C, obtain secondary mixed liquor；
First by positioned at the wavelength regulation of the ultraviolet source of the reactor on right side to 295 nm, then by the secondary mixed liquor and
Chlorine is passed through the reactor positioned at right side and uniformly mixed, and temperature of the regulation in the middle reactor, makes
The mixed once liquid and chlorine react 2~3 h under the conditions of 0.1~0.2 Mpa, 79 DEG C, obtain liquid solid phosgene.
Embodiment 3
The present embodiment provides a kind of method for applying above-mentioned solid phosgene synthesizer to carry out solid phosgene synthesis, and it includes following
Step：
First by positioned at the wavelength regulation of the ultraviolet source of the reactor in left side to 368nm, then by dimethyl carbonate and chlorine
It is passed through in the reactor in left side and uniformly mixes, and temperature of the regulation in the reactor in left side, make carbon
Dimethyl phthalate and chlorine react 3~4 h under the conditions of 0.1~0.2 Mpa, 40 DEG C, obtain mixed once liquid；
First by positioned at the wavelength regulation of the ultraviolet source of the middle reactor to 320 nm, then by the mixed once liquid and
Chlorine is passed through positioned at the middle reactor and uniformly mixed, and temperature of the regulation in the middle reactor, makes
The mixed once liquid and chlorine react 2~3 h under the conditions of 0.1~0.2 Mpa, 60 DEG C, obtain secondary mixed liquor；
First by positioned at the wavelength regulation of the ultraviolet source of the reactor on right side to 290 nm, then by the secondary mixed liquor and
Chlorine is passed through the reactor positioned at right side and uniformly mixed, and temperature of the regulation in the middle reactor, makes
The mixed once liquid and chlorine react 2~3 h under the conditions of 0.1~0.2 Mpa, 85 DEG C, obtain liquid solid phosgene.
Embodiment 4
The present embodiment provides a kind of method for applying above-mentioned solid phosgene synthesizer to carry out solid phosgene synthesis, and it includes following
Step：
First by positioned at the wavelength regulation of the ultraviolet source of the reactor in left side to 385 nm, then by dimethyl carbonate and chlorine
It is passed through in the reactor in left side and uniformly mixes, and temperature of the regulation in the reactor in left side, make carbon
Dimethyl phthalate and chlorine obtain mixed once liquid in 0.1~0.2 Mpa, 45 DEG C of h of conditioned response 3~4；
First by positioned at the wavelength regulation of the ultraviolet source of the middle reactor to 307 nm, then by the mixed once liquid and
Chlorine is passed through positioned at the middle reactor and uniformly mixed, and temperature of the regulation in the middle reactor, makes
The mixed once liquid and chlorine obtain secondary mixed liquor in 0.1~0.2 Mpa, 63 DEG C of 2~3 h of reaction；
First by positioned at the wavelength regulation of the ultraviolet source of the reactor on right side to 285 nm, then by the secondary mixed liquor and
Chlorine is passed through the reactor positioned at right side and uniformly mixed, and temperature of the regulation in the middle reactor, makes
The mixed once liquid and chlorine react 2~3 h under the conditions of 0.1~0.2 Mpa, 88 DEG C, obtain liquid solid phosgene.
Solid phosgene reaches following index made from embodiment 2~4：
| Index name | Mass percent/% |
| Feed stock conversion | ≥99.0 |
| Solid phosgene content | ≥99.0 |
| It is other | ≤1.0 |
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；Although ginseng
The present invention is described in detail according to preferred embodiment, those of ordinary skills in the art should understand that：Still can be with
Embodiment to the present invention is modified or carries out equivalent substitution to some technical characteristics；Without departing from skill of the present invention
The spirit of art scheme, it all should cover among claimed technical scheme scope of the invention.
Claims (9)
1. a kind of solid phosgene synthesizer, it is characterised in that：It includes three reactors being sequentially connected in series from left to right, three
The height of the individual reactor is reduced successively from left to right, each reactor include respectively reactor housing, be arranged at it is described anti-
Answer liquid inlet opening, gas feed mouthful, material outlet and the tail gas outlet of still shell body, for controlling in the reactor
The heat transfer system of the temperature of chamber and adjustable wavelength and the ultraviolet source of power installed in the inner chamber of the reactor, the purple
The wavelength of outer light source is 200~400 nm；Positioned at the liquid inlet opening of the middle reactor and positioned at the described anti-of left side
The material outlet of kettle is answered to be connected；Positioned at the material outlet and the reactor positioned at right side of the middle reactor
Liquid inlet opening be connected.
2. solid phosgene synthesizer according to claim 1, it is characterised in that：The reactor positioned at left side
The wavelength of ultraviolet source is 330~400 nm；It is 300~330 positioned at the wavelength of the ultraviolet source of the middle reactor
nm；It is 280~300 nm positioned at the wavelength of the ultraviolet source of the reactor on right side.
3. solid phosgene synthesizer according to claim 1 or 2, it is characterised in that：The reactor positioned at left side
Inner chamber temperature be 35~50 DEG C；Temperature positioned at the inner chamber of the middle reactor is 50~65 DEG C；Positioned at right side
The temperature of the inner chamber of the reactor is 65~90 DEG C.
4. solid phosgene synthesizer according to claim 3, it is characterised in that：The reactor further comprises installing
Liquid distribution trough in the inner chamber of the reactor, the liquid distribution trough is connected with the liquid inlet opening；Wherein, the liquid
Body distributor includes ring-shaped liquid distributor cavity, and communicate therewith many are evenly distributed with the ring-shaped liquid distributor cavity
Liquid guide flow pipe is installed in individual fluid apertures, the fluid apertures.
5. solid phosgene synthesizer according to claim 4, it is characterised in that：The reactor further comprises installing
Gas distributor in the inner chamber of the reactor, the gas distributor is connected with the gas feed mouthful；Wherein, the gas
Body distributor includes annular gas distributor cavity and the unidirectional outlet being evenly distributed on the annular gas distributor cavity
Pipe, the Unidirectional air outlet pipe includes the escape pipe body being connected with the toroidal cavity of the gas distributor and is arranged at described
The sideboard of the port of export of escape pipe body, the sideboard is hinged with the escape pipe body.
6. solid phosgene synthesizer according to claim 5, it is characterised in that：The reactor also includes being installed on institute
The agitator of reactor housing tip is stated, is connected with the agitator and positioned at the agitating shaft and peace of the inner chamber of the reactor
Loaded on the stirring vane on the agitating shaft.
7. solid phosgene synthesizer according to claim 6, it is characterised in that：The agitating shaft respectively with the liquid
The angle of the straight line extended line of mozzle and the Unidirectional air outlet pipe is 45o。
8. solid phosgene synthesizer according to claim 7, it is characterised in that：The liquid inlet opening and the tail gas
Outlet is respectively arranged at the top of the reactor housing, and the gas feed mouthful and the material outlet are respectively arranged at
The bottom of the reactor housing, and discharged on the outside of the reactor housing with the liquid inlet opening, the tail gas
Mouth, the gas feed are separately installed with control valve on mouthful position corresponding with the material outlet.
9. a kind of solid phosgene synthetic method, it is characterised in that the solid phosgene described in application any one of claim 1~9 is closed
Solid phosgene synthesis is carried out into device, it comprises the following steps：
First by positioned at the wavelength regulation of the ultraviolet source of the reactor in left side to 330~400 nm, then by dimethyl carbonate
It is passed through in the reactor in left side and uniformly mixes with chlorine, and regulation is positioned at the inner chamber of the reactor in left side
Temperature, makes dimethyl carbonate and chlorine react 3~4 h under the conditions of 0.1~0.2 Mpa, 35~50 DEG C, obtains mixed once
Liquid；
First will once it be mixed to 300~330 nm, then by described positioned at the wavelength regulation of the ultraviolet source of the middle reactor
Close liquid and chlorine is passed through positioned at the middle reactor and uniformly mixed, and regulation is positioned at the inner chamber of the middle reactor
Temperature, the mixed once liquid and chlorine is reacted 2~3 h under the conditions of 0.1~0.2 Mpa, 50~65 DEG C, obtain secondary
Mixed liquor；
First by positioned at the wavelength regulation of the ultraviolet source of the reactor on right side to 280~300 nm, then will be described secondary mixed
Close liquid and chlorine is passed through the reactor positioned at right side and uniformly mixed, and regulation is positioned at the inner chamber of the middle reactor
Temperature, make the mixed once liquid and chlorine 0.1~0.2 Mpa, 65~90 DEG C reaction 2~3 h, obtain liquid solid light
Gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710289417.8A CN106984253B (en) | 2017-04-27 | 2017-04-27 | Solid phosgene synthesis device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710289417.8A CN106984253B (en) | 2017-04-27 | 2017-04-27 | Solid phosgene synthesis device and method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106984253A true CN106984253A (en) | 2017-07-28 |
| CN106984253B CN106984253B (en) | 2022-11-22 |
Family
ID=59418203
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710289417.8A Active CN106984253B (en) | 2017-04-27 | 2017-04-27 | Solid phosgene synthesis device and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106984253B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109395683A (en) * | 2018-12-12 | 2019-03-01 | 内蒙古元正精细化工有限责任公司 | A kind of synthesizer and its synthetic method of solid phosgene |
| CN113559812A (en) * | 2021-08-25 | 2021-10-29 | 福建永荣科技有限公司 | Device and method for treating hydrogenation tail gas |
| CN113861028A (en) * | 2021-10-29 | 2021-12-31 | 山西碧洲生物科技股份有限公司 | Process method and device for continuously producing di (trichloromethyl) carbonate |
| CN115945152A (en) * | 2022-12-06 | 2023-04-11 | 安庆亿成化工科技有限公司 | Can prevent metatritoluene oxidation reaction unit of whirl dispersion reactant |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1347870A (en) * | 2000-10-18 | 2002-05-08 | 合肥工业大学 | Triphosgene preparing process |
| US20100093931A1 (en) * | 2008-07-24 | 2010-04-15 | Lanxess Inc. | Process for the continuous hydrogenation of carbon-carbon double bonds in an unsaturated polymer to produce a hydrogenated polymer |
| CN203440266U (en) * | 2013-08-20 | 2014-02-19 | 山西碧春生物科技有限公司 | Triphosgene synthesis reactor |
| CN203790949U (en) * | 2014-05-04 | 2014-08-27 | 杭州百事特实业有限公司 | Methyl capped polyether production device |
| WO2015003595A1 (en) * | 2013-07-09 | 2015-01-15 | 南京奥凯化工科技有限公司 | Preparation method of dichloropropanol |
| CN105112100A (en) * | 2015-08-31 | 2015-12-02 | 宁波镇洋化工发展有限公司 | Continuous production technique of chlorinated paraffin |
| CN105195080A (en) * | 2015-10-10 | 2015-12-30 | 开封华瑞化工新材料股份有限公司 | Synthesis device and method for xylylene diisocynate |
| CN106512869A (en) * | 2016-11-22 | 2017-03-22 | 中国科学院上海高等研究院 | Fluid uniform distribution device with fractal structure |
| CN206778413U (en) * | 2017-04-27 | 2017-12-22 | 平顶山市神鹰化工科技有限公司 | A kind of solid phosgene synthesizer |
-
2017
- 2017-04-27 CN CN201710289417.8A patent/CN106984253B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1347870A (en) * | 2000-10-18 | 2002-05-08 | 合肥工业大学 | Triphosgene preparing process |
| US20100093931A1 (en) * | 2008-07-24 | 2010-04-15 | Lanxess Inc. | Process for the continuous hydrogenation of carbon-carbon double bonds in an unsaturated polymer to produce a hydrogenated polymer |
| WO2015003595A1 (en) * | 2013-07-09 | 2015-01-15 | 南京奥凯化工科技有限公司 | Preparation method of dichloropropanol |
| CN203440266U (en) * | 2013-08-20 | 2014-02-19 | 山西碧春生物科技有限公司 | Triphosgene synthesis reactor |
| CN203790949U (en) * | 2014-05-04 | 2014-08-27 | 杭州百事特实业有限公司 | Methyl capped polyether production device |
| CN105112100A (en) * | 2015-08-31 | 2015-12-02 | 宁波镇洋化工发展有限公司 | Continuous production technique of chlorinated paraffin |
| CN105195080A (en) * | 2015-10-10 | 2015-12-30 | 开封华瑞化工新材料股份有限公司 | Synthesis device and method for xylylene diisocynate |
| CN106512869A (en) * | 2016-11-22 | 2017-03-22 | 中国科学院上海高等研究院 | Fluid uniform distribution device with fractal structure |
| CN206778413U (en) * | 2017-04-27 | 2017-12-22 | 平顶山市神鹰化工科技有限公司 | A kind of solid phosgene synthesizer |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109395683A (en) * | 2018-12-12 | 2019-03-01 | 内蒙古元正精细化工有限责任公司 | A kind of synthesizer and its synthetic method of solid phosgene |
| CN113559812A (en) * | 2021-08-25 | 2021-10-29 | 福建永荣科技有限公司 | Device and method for treating hydrogenation tail gas |
| CN113559812B (en) * | 2021-08-25 | 2022-09-16 | 福建永荣科技有限公司 | Device and method for treating hydrogenation tail gas |
| CN113861028A (en) * | 2021-10-29 | 2021-12-31 | 山西碧洲生物科技股份有限公司 | Process method and device for continuously producing di (trichloromethyl) carbonate |
| CN115945152A (en) * | 2022-12-06 | 2023-04-11 | 安庆亿成化工科技有限公司 | Can prevent metatritoluene oxidation reaction unit of whirl dispersion reactant |
| CN115945152B (en) * | 2022-12-06 | 2023-07-04 | 安庆亿成化工科技有限公司 | Trimellitic oxidation reaction device capable of preventing cyclone dispersion reactant |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106984253B (en) | 2022-11-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106984253A (en) | A kind of solid phosgene synthesizer and method | |
| CN106552577B (en) | A kind of multilayer guide shell bubbling reactor and its application method | |
| CN208218740U (en) | Propylene polymerization combination evaluation device | |
| CN105195080B (en) | The synthesizer and method of XDI | |
| CN206778413U (en) | A kind of solid phosgene synthesizer | |
| CN106540642A (en) | Light-initiated controlled radical polymerization device and application | |
| CN104689763B (en) | Oxidizing reaction device and use of oxidizing reaction device | |
| CN206082502U (en) | Modular mix reation kettle in advance | |
| CN207493676U (en) | Continuous photochemical reaction unit and system | |
| CN105233764B (en) | Ventilation device and radial reactor | |
| CN208771389U (en) | Continuous reaction apparatus and system | |
| CN105233762B (en) | Methanol synthesis reaction system and methanol synthesis reaction method | |
| CN109395683A (en) | A kind of synthesizer and its synthetic method of solid phosgene | |
| CN205517782U (en) | Automatic esterifying kettle of stirring | |
| CN211913740U (en) | Solid phosgene's synthesizer | |
| CN209465014U (en) | A kind of synthesizer of solid phosgene | |
| CN101766980A (en) | Reactor for preparing tetrabromoethane by addition reaction of bromine and acetylene and synthesis process | |
| CN106000267B (en) | A kind of adipic acid synthesizer and its application method | |
| CN202893350U (en) | Polyether reaction kettle | |
| CN105218310B (en) | Methanol synthesis reaction device and methanol synthesis reaction method | |
| CN101607878B (en) | Device for preparing fluorenone by means of liquid phase oxidation and preparation method thereof | |
| CN101733057B (en) | Built-in cooling type point light source photo-chemical integrated reactor with | |
| CN206652499U (en) | A kind of self-suction mixing reactor | |
| CN201815298U (en) | Reactor for preparing ethylene by dehydrating ethanol | |
| CN106543297B (en) | A kind of polymerization of bimodal polyethylene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |